CN104513985A - Nickel-chromium alloy metallographic corrosion solution and corrosion method - Google Patents
Nickel-chromium alloy metallographic corrosion solution and corrosion method Download PDFInfo
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Abstract
The invention relates to a nickel-chromium alloy metallographic corrosion solution and a corrosion method. The corrosion solution is a mixed solution of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water in a volume ratio of 1:1:1:1. The concrete steps include: (1) preparing the corrosion solution, firstly adding water into a container, then adding concentrated nitric acid, concentrated hydrochloric acid and glacial acetic acid respectively, conducting stirring and then performing standing for 10-20min; (2) dripping the corrosion solution on the corrosion surface of a ground and polished nickel-chromium alloy metallographic sample, immersing the sample into the corrosion solution to a depth of 1-2mm, and controlling the corrosion time at 10s-10min; (3) flushing the sample surface with distilled water for more than 2min; and (4) flushing the sample surface with alcohol, and then wiping the sample surface with alcohol-carrying absorbent cotton. According to the invention, the corroded metallographic sample has obvious grain contrast and clear grain boundary line, and at the same time, the defects of under-corrosion and over-corrosion can be avoided. The corrosion solution can rapidly and efficiently corrode the metallographic structure of the sample.
Description
Technical field
The present invention relates to nichrome metallurgical analysis technical field, be specifically related to a kind of nichrome metallographic etchant and caustic solution.
Background technology
Metallurgical analysis is a kind of routine inspection method evaluating metallic substance quality according to related standards and regulation.In rolling metal processing, metallurgical analysis and metallographic structure are observed and are played very important effect, can be observed phase composite and each phase grain size and nonmetallic compound slag inclusion in the alloy be corroded, burning or the defect such as overheated by metallographic structure.Metallurgical analysis also can be used to judge that whether product processes is perfect, helps to seek product defects Producing reason and by metallurgical analysis optimized production process parameter.Thus metallurgical analysis is produced and requisite a kind of detection means in scientific research.
Metallurgical analysis plays very important effect in rolling metal processing, and the producing of metallurgical analysis sample, grinding and polishing, corrosion are also very important important steps.Carry out metallographic structure and Observation of Defects thereof, first want grinding and polishing to go out no marking, be pasted onto the qualified metallographic specimen on metallographic specimen surface without lapping paste, then carry out the surface corrosion of sample.In corrosive fluid preparation, the selection of acid and the configuration proportion of various acid and water are the key elements of corrosive fluid proportioning.The metallographic specimen of heterogeneity, its acid-resistant corrosion difference is large especially, and corrosive fluid preparation and configuration proportion difference, etching time is different.Etching pit requires extremely strict, if the configuration proportion of various acid is not in place in corrosive fluid, basic corrosion does not go out the phase constitution of sample; If the configuration proportion of acid is too high in corrosive fluid, easily form excessive erosion, crystal boundary and grain formation a slice black, do not observe crystal boundary and grain size clearly at all, do not observe contrast between phase and phase yet.
The nichrome large usage quantity that the whole nation is annual, the enterprise producing nichrome gets more and more, and along with market competition is growing more intense, client is more and more strict to the performance requriements of product.Want to establish oneself in an unassailable position in the market competition of fierceness, promoting nichrome quality product is key link.
Utilize advanced detection method, nichrome quality product is analyzed and passed judgment on.And in all physics, chemical detection, metallurgical analysis is particularly crucial a kind of detection method.By metallurgical analysis, measure and grasp the grain fineness number of product, judging that whether temperature of fusion is reasonable, judging in the product of production, whether with or without slag inclusion, nonmetal oxide, crackle, burning and the defect such as overheated, to judge that whether follow-up complete processing is reasonable.
From the data display can found at present, the corrosion data of Ni-based ultrafine powder metallographic specimen is considerably less, and according to finding the corrosion carrying out this nickelalloy metallographic specimen about the configuration proportion of nichrome metallographic liquid making method and various corrosive fluid, exist a lot of not enough.The corrosive fluid configured according to a certain percentage according to nitric acid and water or nitric acid, hydrochloric acid and water carries out the corrosion of nichrome metallographic specimen, first etching time is longer, second corrosive effect is not obvious, does not see metallographic structure clearly, and the crystal boundary line in metallographic structure between crystal grain is unintelligible; If increase nitric acid or nitric acid and hydrochloric acid ratio, formation excessive erosion, all there is black in crystal boundary and crystal grain, does not observe metallurgical structure clearly.So will observe metallographic structure clearly, make different alternately have obvious line of delimitation and contrast, the preparation of corrosive fluid is extremely crucial.
Summary of the invention
For the deficiency of above-mentioned prior art, the invention provides a kind of nichrome metallographic etchant and caustic solution, the metallographic specimen after corrosion can be made to obtain gem-pure metallographic structure.
The present invention is achieved by the following technical solutions:
A kind of nichrome metallographic etchant, it is characterized in that this corrosive fluid is the mixing solutions of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water, in mixing solutions, the volume ratio of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water is 1:1:1:1.
A kind of nichrome metallographic etchant, it is characterized in that the mass percent concentration of described concentrated nitric acid is 65 ~ 68%, the mass percent concentration of concentrated hydrochloric acid is 36 ~ 38%, and the mass percent concentration of glacial acetic acid is greater than 99.5%.
The method using above-mentioned corrosive fluid to corrode nichrome metallographic specimen, is characterized in that, said method comprising the steps of:
(1) prepare corrosive fluid, first add water in a reservoir, then add concentrated nitric acid, concentrated hydrochloric acid and glacial acetic acid respectively, after stirring, leave standstill 10 ~ 20min;
(2) dropped in by corrosive fluid on the erosional surface of the nichrome metallographic specimen after grinding and polishing, it is 1-2mm that corrosive fluid immerses sample depth, and etching time is 10s ~ 10min;
(3) distilled water flushing specimen surface is used, flush time more than 2 minutes;
(4) alcohol rinse specimen surface is used, then with the absorbent cotton wiping specimen surface of band alcohol.
The method using above-mentioned corrosive fluid to corrode nichrome metallographic specimen, is characterized in that, the etching time of step (2) is 10s ~ 60s.
The method using above-mentioned corrosive fluid to corrode nichrome metallographic specimen, is characterized in that, the etching time of step (2) is 5min ~ 10min.
Advantageous Effects of the present invention, the invention provides a kind of nichrome metallographic etchant and caustic solution, by the corrosive fluid that concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water are made according to certain volume ratio, to nichrome etching pit, make grain contrast in the metallographic specimen after excessive erosion obvious, crystal boundary line is clear, and avoid corrosion deficiency and excessive erosion defect, this corrosive fluid can erode away the metallographic structure of sample fast and efficiently simultaneously.
Accompanying drawing explanation
Fig. 1 is the nichrome metallographic specimen 1 after using corrosive fluid of the present invention to corrode.
Fig. 2 is the nichrome metallographic specimen 2 after using corrosive fluid of the present invention to corrode.
Fig. 3 is the nichrome metallographic specimen 1 scanning electron microscope result figure after corroding use corrosive fluid of the present invention.
Fig. 4 is the nichrome metallographic specimen 2 scanning electron microscope result figure after corroding use corrosive fluid of the present invention.
Fig. 5 is the detected result figure of the nichrome metallographic specimen 1 after using corrosive fluid of the present invention to corrode.
Fig. 6 is the detected result figure of the nichrome metallographic specimen 2 after using corrosive fluid of the present invention to corrode.
Embodiment
A kind of nichrome metallographic etchant of the present invention, this corrosive fluid is the mixing solutions of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water, in mixing solutions, the volume ratio of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water is 1:1:1:1, wherein the mass percent concentration of concentrated nitric acid is 65 ~ 68%, the mass percent concentration of concentrated hydrochloric acid is 36 ~ 38%, and the mass percent concentration of glacial acetic acid is greater than 99.5%.
The method using above-mentioned corrosive fluid to corrode nichrome metallographic specimen, comprises the following steps:
(1) prepare corrosive fluid, first add water in a reservoir, then add concentrated nitric acid, concentrated hydrochloric acid and glacial acetic acid respectively, after stirring, leave standstill 10 ~ 20min;
(2) then suck corrosive fluid with plastic dropper to be dropped on the erosional surface of the nichrome metallographic specimen after grinding and polishing by corrosive fluid, make it evenly be capped at specimen surface, corrosive fluid covers sample depth for being 1-2mm, and etching time is 10s ~ 10min;
(3), after corrosion, clamp the both sides of sample with iron clamp, use distilled water flushing specimen surface, flush time more than 2 minutes;
(4) use alcohol rinse specimen surface, then with the absorbent cotton wiping specimen surface of band alcohol, to prevent residual acid oxidase specimen surface, then utilize metaloscope to carry out metallographic microstructure observation and Grain size analysis.
Etching time is relevant to the complete processing of sample, if casting state and hot-work sample, etching time is shorter, and etching time is 10s ~ 60s; If cold working state sample, crystal grain is tiny, and organize dense, good corrosion resistance, etching time is longer, and excellent etching time is 5min ~ 10min.
Embodiment 1
Be 1:1:1:1 according to the volume ratio of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water, first add 50ml water in a reservoir, add 50ml concentrated nitric acid, 50ml concentrated hydrochloric acid and 50ml glacial acetic acid more respectively, 10 minutes are left standstill after stirring, wherein concentrated nitric acid mass percent concentration is 65%, the mass percent concentration of concentrated hydrochloric acid is 36%, and the mass percent concentration of glacial acetic acid is 99.6%.Then 2080 nichrome bars (composition is as shown in table 1 below) are got, then Linear cut is utilized to carry out metallographic specimen sampling, make the metallographic specimen of 20mm*20mm*15mm, the waterproof abrasive paper of different thicknesses is utilized to grind, as 400 orders, 600 orders, 800 orders, 1000 orders, 1500 orders, 2000 object silicon carbide papers carry out grind away.The grinding and polishing quality of metallographic specimen directly affects etching pit result and metallographic structure analysis.First the key link of thus carrying out metallurgical analysis is the preparation of sample.Utilize 400 object sand paper to carry out grind away, rinse with water after milled, observe specimen surface cut and whether entirely disappear.Observational technique is as follows: hand-held sample, first observe from specimen surface and canthus sight line 90 degree, if do not observe cut, then hand-held sample slowly rotates, rotation limit, limit is from the cut of different angle views specimen surfaces, till specimen surface is substantially parallel with viewing angle, if all no marking can change sand paper, if there is cut to continue mill.
Table 1 2080 nichrome chemical composition
During with 400 order-1000 order abrasive paper for metallograph metallic phase polishing, the rotating speed of polished machine is set to 500-550 and turns/min, due to flint paper grind time, the cut of specimen surface is comparatively dark, can the cut of cancellation specimen surface when only having rotating speed fast; When adopting 1200-1500 object abrasive paper for metallograph to grind, now metallographic specimen surface is more smooth, if when selecting quick rotating speed, the cut that easy formation is new, the rotating speed of polished machine is set to 400-450 and turns/min, when adopting 2000 object abrasive paper for metallograph to carry out grinding and polishing, the rotating speed of metallographical polishing machine is that 350-400 turns/min; Utilize diamond paste polishing on polished machine.Diamond paste also has W0.5 micron, W1.5 micron, W3.5 micron and W5 micron, after first selecting the diamond paste of W5 micron to carry out polishing 1min, the diamond paste of W3.5 micron is selected to carry out grinding and polishing 30-50s again, then the diamond paste of W0.5 micron is selected to carry out after polishing is about 1min, observe the very bright cunning of specimen surface, without any cut, then change clean polishing cloth, with alcohol as lubricant, the lapping paste of specimen surface of just can skimming after polishing 1-2min.Then first rinse specimen surface with water, then use alcohol rinse specimen surface.
Corrode with the corrosive fluid prepared, it is 1mm that corrosive fluid immerses sample depth, and etching time is 10 seconds, then with distilled water or alcohol rinse specimen surface 2.3min, uses metaloscope metallographicobservation.
Embodiment 2
Be 1:1:1:1 according to the volume ratio of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water, first add 55ml water in a reservoir, add 55ml concentrated nitric acid, 55ml concentrated hydrochloric acid and 55ml glacial acetic acid more respectively, 20 minutes are left standstill after stirring, wherein concentrated nitric acid mass percent concentration is 68%, the mass percent concentration of concentrated hydrochloric acid is 38%, the mass percent concentration of glacial acetic acid is 99.9%, get nichrome sample to corrode, it is 2mm that corrosive fluid immerses sample depth, etching time is 60 seconds, then with distilled water or alcohol rinse specimen surface, uses metaloscope metallographicobservation.
Embodiment 3
According to concentrated nitric acid, concentrated hydrochloric acid, the volume ratio of glacial acetic acid and water is 1:1:1:1, first add 50ml water in a reservoir, add 50ml concentrated nitric acid respectively again, 50ml concentrated hydrochloric acid and 50ml glacial acetic acid, 15 minutes are left standstill after stirring, wherein concentrated nitric acid mass percent concentration is 67%, the mass percent concentration of concentrated hydrochloric acid is 37%, the mass percent concentration of glacial acetic acid is 99.8%, get nichrome sample to corrode, it is 2mm that corrosive fluid immerses sample depth, etching time is 5min, again with distilled water or alcohol rinse specimen surface 2.5min, use metaloscope metallographicobservation.
Embodiment 4
According to concentrated nitric acid, concentrated hydrochloric acid, the volume ratio of glacial acetic acid and water is 1:1:1:1, first add 50ml water in a reservoir, add 50ml concentrated nitric acid respectively again, 50ml concentrated hydrochloric acid and 50ml glacial acetic acid, 18 minutes are left standstill after stirring, wherein concentrated nitric acid mass percent concentration is 67%, the mass percent concentration of concentrated hydrochloric acid is 38%, the mass percent concentration of glacial acetic acid is 99.8%, get nichrome sample to corrode, it is 1.5mm that corrosive fluid immerses sample depth, etching time is 10min, again with distilled water or alcohol rinse specimen surface 3min, use metaloscope metallographicobservation.
As shown in Figure 1, some stains can be seen after corrosion, in order to confirm whether stain is excessive erosion or lapping paste, hereby done scanning electron microscope, result as shown in Figure 2, for understanding fully the chemical composition of stain, stain in Fig. 2 is got ready, result is got ready: the chemical composition of stain is mainly the oxide compound of Si and the compound of nickel and iron, non-ground cream, so these stains are product defects as can be seen from Fig. 3 stain.
Note: this corrosive fluid is acid strong, and corrosion need be carried out in stink cupboard, need wear acid-proof gloves and mouth mask when carrying out etching pit operation.
Claims (5)
1. a nichrome metallographic etchant, is characterized in that this corrosive fluid is the mixing solutions of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water, and in mixing solutions, the volume ratio of concentrated nitric acid, concentrated hydrochloric acid, glacial acetic acid and water is 1:1:1:1.
2. a kind of nichrome metallographic etchant according to claim 1, is characterized in that the mass percent concentration of described concentrated nitric acid is 65 ~ 68%, and the mass percent concentration of concentrated hydrochloric acid is 36 ~ 38%, and the mass percent concentration of glacial acetic acid is greater than 99.5%.
3. the method using the corrosive fluid described in claim 1 or 2 to corrode nichrome metallographic specimen, is characterized in that, said method comprising the steps of:
(1) prepare corrosive fluid, first add water in a reservoir, then add concentrated nitric acid, concentrated hydrochloric acid and glacial acetic acid respectively, after stirring, leave standstill 10 ~ 20min;
(2) dropped in by corrosive fluid on the erosional surface of the nichrome metallographic specimen after grinding and polishing, it is 1-2mm that corrosive fluid immerses sample depth, and etching time is 10s ~ 10min;
(3) distilled water flushing specimen surface is used, flush time more than 2 minutes;
(4) alcohol rinse specimen surface is used, then with the absorbent cotton wiping specimen surface of band alcohol.
4. a kind of method using above-mentioned corrosive fluid to corrode nichrome metallographic specimen according to claim 3, is characterized in that, the etching time of step (2) is 10s ~ 60s.
5. a kind of method using above-mentioned corrosive fluid to corrode nichrome metallographic specimen according to claim 3, is characterized in that, the etching time of step (2) is 5min ~ 10min.
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| CN105018931A (en) * | 2015-07-24 | 2015-11-04 | 金川集团股份有限公司 | GH3030 high-temperature alloy as-cast metallographic etchant and preparing method and using method thereof |
| CN105018932A (en) * | 2015-07-24 | 2015-11-04 | 金川集团股份有限公司 | Ni80Cr20 alloy rolled plate metallographic corrosive liquid and preparation method and use method thereof |
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| CN105018931A (en) * | 2015-07-24 | 2015-11-04 | 金川集团股份有限公司 | GH3030 high-temperature alloy as-cast metallographic etchant and preparing method and using method thereof |
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| CN105256315A (en) * | 2015-09-16 | 2016-01-20 | 昆山全亚冠环保科技有限公司 | Metallographic corrosive agent and method for nickel-vanadium alloy |
| CN105177577A (en) * | 2015-09-30 | 2015-12-23 | 金川集团股份有限公司 | Corrosion method for small-specification red copper rod |
| CN105241885A (en) * | 2015-09-30 | 2016-01-13 | 金川集团股份有限公司 | Forged magnetically soft alloy 1J50 alloy metallographic corrosive liquid and applications thereof |
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| CN107286939A (en) * | 2017-06-19 | 2017-10-24 | 江阴润玛电子材料股份有限公司 | A kind of semiconductor chip nickeline corrosive liquid |
| CN109540634A (en) * | 2018-11-20 | 2019-03-29 | 中国航发贵州黎阳航空动力有限公司 | A kind of detection method for GH4648 sheet coupon crystal grain and microscopic structure |
| CN110132696A (en) * | 2019-06-04 | 2019-08-16 | 天津中德应用技术大学 | A kind of etching pit method of high temperature alloy |
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| CN111662717B (en) * | 2020-07-14 | 2021-08-31 | 北京航空航天大学宁波创新研究院 | Metallographic corrosive liquid of bismuth selenide material and metallographic display method |
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| CN111850563B (en) * | 2020-07-30 | 2022-04-12 | 北京钢研高纳科技股份有限公司 | Rapid detection method for surface structure of nickel-based superalloy forging and high-power structure corrosion liquid |
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